EP2457086B1 - Procédé et dispositif permettant de préparer des substances pour des analyses quantitatives et qualitatives - Google Patents

Procédé et dispositif permettant de préparer des substances pour des analyses quantitatives et qualitatives Download PDF

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Publication number
EP2457086B1
EP2457086B1 EP10745001.7A EP10745001A EP2457086B1 EP 2457086 B1 EP2457086 B1 EP 2457086B1 EP 10745001 A EP10745001 A EP 10745001A EP 2457086 B1 EP2457086 B1 EP 2457086B1
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European Patent Office
Prior art keywords
sealing edge
head
counter
sample
cavity
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EP10745001.7A
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German (de)
English (en)
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EP2457086A1 (fr
Inventor
Matthias Loppacher
Eike Reich
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CAMAG
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CAMAG
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1095—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N2030/009—Extraction

Definitions

  • the present invention relates to a method for the preparation of substances for qualitative and quantitative analyzes according to the preamble of patent claim 1 and an apparatus for carrying out the method according to the preamble of claim 6.
  • ballast in connection with the measurement in the analyzer, they impede an accurate measurement.
  • the present method and the device presented here are based on the findings obtained in the methods of thin-layer chromatography.
  • the DE10036293A1 von Lucasmann describes a device with which samples can be isolated.
  • the US 5,208,458 von Busch presents a method and a device with which defined samples can be taken from gel. It has been shown, however, that the idea of Busch, which underlies his patent, can not be realized in practice in gel applications.
  • the present invention now has the object of a method and apparatus for the preparation of substances for qualitative and quantitative analyzes of the type mentioned for liquid, highly viscous, dried, coagulated or thickened, present in solid form, biologically active dried, or offset for stabilization with protective colloids
  • the substance sought is usually embedded in a matrix.
  • This matrix can consist of insoluble solid or soluble constituents.
  • the presented method sets itself the goal of "washing out” the sought-after substance - the analyte - from the samples and, together with the entrained or dissolved matrix, the added liquid and possibly an internal standard as sample, to the measuring instrument. Depending on the composition of the sample, this is done by simply washing out, dissolving or extracting.
  • the substance is dissolved out of the matrix, so that they together with the liquid, eg. B. a solvent or extractant the meter, z. B. can be supplied to the spectrometer.
  • the first step of the method is that with the device described later, a defined region of the sample from the environment in a cavity 3 (FIG. Fig. 1 ) is enclosed and isolated. The most important part of the seal thereby get the sealing edges 4 and 5. Between the sealing edges 4,5 but also material of the samples 11 is squeezed together ( Fig. 2 ) to achieve improved tightness.
  • a small but sufficient amount of liquid is then added to the now closed space, which comes into contact with the sample in the closed cavity 3.
  • this liquid can either be rinsed out, dissolved or extracted directly, or a softening process must precede the rinsing out.
  • the liquid with the sample is left in the closed area together with the sample for a certain time and then rinsed out as a pattern.
  • the time required for softening depends on the properties of the sample, the liquid and the substance but is usually in the range of 1-60 seconds.
  • the type of sample, the liquid and the substance are also dependent on whether it is possible to wash it out directly, or to initiate a solution or extraction process.
  • the presented procedure allows all possibilities. For each substance, a laboratory test determines the type and amount of liquid to be supplied and what process is necessary to prepare the substance so that it can later be transported in a liquid state and allow the measurement of accurate analysis values.
  • the aim of the preceding steps is to deliver a highly concentrated fraction of the substance to the meter via the lead 9, dissolved in or mixed with the clearly defined liquid. This is called “pattern” here.
  • pattern One would like to "take away” as few disturbing parts of the matrix to the measuring device.
  • the mixture of the extracted or dissolved substance is pushed out of the isolated cavity 3 in a plug shape and fed to the measuring instrument. It is important that the paths are short and the substance is brought as directly as possible to the measuring point.
  • the necessary amount, time and the sequence of process steps can be very different depending on the sample and its matrix. They are defined and defined empirically as described above.
  • the decisive phase in the method described above takes place when the device is closed, that is to say when the head 1 of the device forms a unit with the counterhead 2 and stands on one another ( Fig. 1 ).
  • the sealing edge 4 of the head 1 forms with the counter-sealing edge 5 of the counterhead 5 and the material of the sample 11, which is clamped between the two sealing edges 4.5 a completely closed cavity 3.
  • this cavity 3 can via a supply line 8, a liquid, for example a Rinsing, solvent or extractant are supplied. Material that is in the cavity 3 can leave this only via the discharge line 9. This happens when the cavity 3 is filled and is introduced by supply line 8 of new liquid.
  • the supply line 8 is arranged at one "end" of the cavity 3 and the discharge line 9 at the other "end".
  • the lead 8 and the lead 9 are located at the farthest tangents of the cylinder.
  • the arrangement which is determined empirically for the materials to be tested, must be such that in the cavity 3 as possible no, or if desired targeted mixing takes place.
  • the described arrangement of lead 8 and derivative 9 represents only one possible embodiment. There may also be other variants such as, for example, coaxial arrangement with central supply line and external discharge, or else several supply and / or discharge lines.
  • sealing edge 4 and the counter-sealing edge 5 in the illustrated elevation form a straight line. This is not necessarily the case in practice.
  • the sealing line between the sealing edge 4 and counter-sealing edge 5 can describe any desired curve, both in plan view and spatially. The two must in the closed state, ie when the head 1 with sealing edge 4 and the counterhead 2 with counter-sealing edge 5 lie on each other, uniformly seal the cavity 3 over the entire sealing line.
  • the term "sealing edges” is mentioned here, they may also be of a planar design, or may even be designed as interlocking profiles.
  • the absolute tightness and insulation of the cavity 3 is achieved in that between the sealing edge 4 and counter-sealing edge 5 material of the sample 11 is clamped and acts as a "sealant" ( Fig. 4 ).
  • a "sealing edge” a conventional seal such as an O-ring with round or polygonal cross-section can be used.
  • this sealing line has a spatially adapted curve.
  • Another embodiment may also be a conical / convex shape.
  • the counterhead 2 represents a flat surface on which the sealing edge 4 as in Fig. 1 exemplified a cavity 3 seals.
  • the device offers the possibility of adapting the method to the samples, substances and carrier liquids. It can be achieved with only partially full cavity 3 a flow ie washing out at the surface. Similarly, the room can be completely filled, for example, avoiding "channeling", what for the softening process described above is essential for a solubilization and an extraction process.
  • Samples 11 are often present for testing in the form of substance spots, on ductile or rigid plates 10, the sample optionally being contained in a chromatographic layer applied to the plate.
  • Fig. 2 shows how a sample 11 which is located on a plate 10, between the head 1 and counter-head 2 is introduced into the device.
  • the sealing edge 4 defines on the thin-layer plate 10 from the cavity 3, in which then is to be dissolved or extracted substance sample. Between the sealing edge 4 of the head 1 and the plate 10 and material of the sample 11 and / or the chromatographic layer is clamped. This acts in many cases in addition to a seal and thus helps to seal the cavity 3 optimally.
  • Samples 11 which have a certain inherent strength such. B. microscopic sections, can also be inserted directly between the head 1 and 2 counter head. Substance samples 11 applied to an absorbent paper can also be processed in exactly the same way.
  • a filter In devices according to Fig. 1 and Fig. 2 it is usually necessary to install a filter, called a "frit", in the lead 9. Different filters are needed for different samples and substances. Another idea is therefore the attachment of a filter 18, which is inserted between substance sample 11 and head 1 ( Fig. 3 ). To avoid the tedious insertion of filter 18 can, for. Example, a device can be selected which leads from a filter roll 20, the filter 18 under the head 1 through the filter roll 20 '. For each new sample 11 is then rotated on the filter roll 20 ', so that new filter 18 under the head 1 ( Fig. 4 ) comes to rest. For the execution of the filter 18 are also more Shapes, such. B.
  • a second device ( Fig. 3 ), which is referred to here in the present case with film 19.
  • This may or may not be the same filter 18.
  • this film 19 is guided by a roller 21 via the counter-head 2 on a roller 21.
  • Film 19 and / or filter 18 may be treated with a typical "internal standard", such as with an isotope of the active ingredient or other reference substances in a defined amount, so that a calibration measurement of the defined isotope is made simultaneously with the measurement of the substance and can be compared.
  • the film 19 is preferably made of impermeable material, while in the embodiment according to Fig. 6 a permeable film 19 must be used.
  • the filter 18 will be made of permeable material, perforated or perforated during use to be permeable to the liquid.
  • Fig. 3 is further shown as filters 18 by means of rollers 20, 20 'and Slide 19 by means of rollers 21, 21 'for the processing of each new sample 11 can be retracted.
  • the filter 18 can also be impregnated with a so-called "internal standard", which is then washed out with the liquid supplied and fed as an additive in the sample to the measuring device.
  • Both filter 18 and foil 19 can take over the function of a ductile or elastic seal if necessary.
  • sealing edge 4 and counter-sealing edge 5, together with filter 18, foil 19 and sample 11, can together ensure the sealing.
  • sealing edge 4 and counter-sealing edge 5 can also be profile and counter profile, the function of which is similar to a labyrinth seal, which then produce by qequetschte parts of the sample 11, the absolute tightness.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Claims (19)

  1. Procédé permettant de préparer des substances pour des analyses qualitatives et quantitatives
    caractérisé en ce que
    dans une cavité (3) confinée et hermétique, une région définie d'un échantillon (11) avec un analyte désiré est pressée et isolée, puis mise en contact avec un liquide introduit via une conduite d'alimentation (8), ce liquide étant acheminé conjointement avec des morceaux de matrice entraînés ou dissous ainsi qu'avec l'analyte désiré, sous une forme appelée spécimen, à travers une conduite d'évacuation (9) à un appareil de mesure,
    dans lequel la cavité (3) est confinée entre une tête (1) avec une arête d'étanchéité (3) et une contre-tête (2) avec une contre-arête d'étanchéité (5) ou entre une tête (1) avec une arête d'étanchéité (3) et une plaque (10) disposée la tête (1) et la contre-tête (2), et
    dans lequel l'herméticité et l'isolation absolue de la cavité (3) sont atteintes en ce que le matériau de l'échantillon (11) est pincé entre l'arête d'étanchéité (4) et la contre-arête d'étanchéité (5) ou entre l'arête d'étanchéité (4) et la plaque (10), et en ce que l'arête d'étanchéité (4) et la contre-arête d'étanchéité (5) s'emboîtent l'une sur l'autre dans l'état fermé, ou en ce que l'arête d'étanchéité (4) et la plaque (10) reposent à plat l'une sur l'autre dans l'état fermé.
  2. Procédé selon la revendication 1,
    caractérisé en ce que
    le liquide introduit coule par-dessus l'échantillon (11).
  3. Procédé selon la revendication 1,
    caractérisé en ce que
    le liquide introduit coule à travers l'échantillon (11).
  4. Procédé selon la revendication 1,
    caractérisé en ce que
    le liquide introduit, avant de couler par-dessus ou à travers, reste dans la cavité (3) avec l'échantillon (11) pendant 1 à 60 secondes, le liquide agissant sur l'échantillon (11) pendant ce temps, le spécimen étant ensuite acheminé par la conduite d'évacuation (9) à l'appareil de mesure.
  5. Procédé selon l'une des revendications précédentes,
    caractérisé en ce que
    un étalon interne est ajouté au spécimen dans la cavité, le spécimen et l'étalon interne étant acheminés ensemble via la conduite d'évacuation (9) à l'appareil de mesure.
  6. Dispositif permettant la mise en oeuvre du procédé selon la revendication 1, avec une tête (1) qui, conjointement avec une contre-tête (2) ou conjointement avec une plaque (10) disposée entre la tête (1) et la contre-tête (2), forme une cavité (3) entourée par une arête d'étanchéité (4), ladite cavité (3) étant pourvue d'une conduite d'alimentation (8) et d'une conduite d'évacuation (9), caractérisé en ce que
    la cavité (3) est, dans l'état fermé, entourée par une ligne d'étanchéité formée par l'arête d'étanchéité (4) de la tête (1) et la contre-arête d'étanchéité (5) de la contre-tête (2) ou par l'arête d'étanchéité (4) et la plaque (10), lesdites arête d'étanchéité (4) et contre-arête d'étanchéité (5) s'emboîtant l'une sur l'autre dans l'état fermé ou l'arête d'étanchéité (4) et la plaque (10) reposant à plat l'une sur l'autre dans l'état fermé, de sorte que la tête (1) et la contre-tête (2) ou la tête (1) et la plaque (10) forment dans l'état assemblé une cavité (3) complètement fermée et isolée de l'extérieur,
    dans lequel l'herméticité et l'isolation absolue de la cavité (3) sont atteintes en ce que le matériau de l'échantillon (11) est pincé entre l'arête d'étanchéité (4) et la contre-arête d'étanchéité (5) ou entre l'arête d'étanchéité (4) et la plaque (10) et une région définie de l'échantillon (11) est enfermée et isolée de l'environnement à l'intérieur de la cavité (3).
  7. Dispositif selon la revendication 6,
    caractérisé en ce que
    la contre-tête (2) est une surface plane, l'arête d'étanchéité (4) et la contre-arête d'étanchéité (5) ayant donc une surface d'étanchéité plane.
  8. Appareil selon la revendication 6,
    caractérisé en ce que
    l'arête d'étanchéité (4) et la contre-arête d'étanchéité (5) ont un profil et contre-profil quelconques qui se correspondent l'un à l'autre de manière à pouvoir s'emboîter.
  9. Dispositif selon la revendication 6,
    caractérisé en ce que
    la conduite d'alimentation (8) et la conduite d'évacuation (9) sont disposées sur le pourtour extérieur de la cavité (3) et l'une en face de l'autre.
  10. Dispositif selon la revendication 6,
    caractérisé en ce que
    en ce que la cavité (3) est conçue de manière à présenter une section A entre la conduite d'alimentation (8) et la conduite d'évacuation (9).
  11. Dispositif selon la revendication 6,
    caractérisé en ce que
    la plaque (10) est en verre, le matériau de l'échantillon (11) étant pincé entre l'arête d'étanchéité (4) et la plaque (10).
  12. Dispositif selon la revendication 6,
    caractérisé en ce que
    la plaque (10) est une plaque ductile (10) dans laquelle le bord d'étanchéité (4) pénètre légèrement.
  13. Dispositif selon la revendication 6,
    caractérisé en ce que
    un échantillon (11) est disposé directement entre la tête (1) et la contre-tête (2).
  14. Dispositif selon la revendication 6,
    caractérisé en ce que
    un filtre (18) est inséré entre l'échantillon (11) et la tête (1).
  15. Dispositif selon la revendication 14,
    caractérisé en ce que
    le filtre (18) est imprégné d'un étalon interne.
  16. Dispositif selon la revendication 6,
    caractérisé en ce que
    un film est inséré entre l'échantillon (11) et la contre-tête (2).
  17. Dispositif selon la revendication 6,
    caractérisé en ce que
    l'arête d'étanchéité (4) est munie d'un joint torique.
  18. Dispositif selon la revendication 6,
    caractérisé en ce que
    la contre-arête d'étanchéité (5) est munie d'un joint torique.
  19. Dispositif selon la revendication 6,
    caractérisé en ce que
    la conduite d'alimentation (8) est située dans dans la tête (1) et la conduite d'évacuation (9) dans la contre-tête (2).
EP10745001.7A 2009-07-24 2010-07-16 Procédé et dispositif permettant de préparer des substances pour des analyses quantitatives et qualitatives Active EP2457086B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH01166/09A CH701526B1 (de) 2009-07-24 2009-07-24 Verfahren und Vorrichtung zur Vorbereitung von Substanzen für qualitative und quantitative Analysen.
PCT/IB2010/053262 WO2011010265A1 (fr) 2009-07-24 2010-07-16 Procédé et dispositif permettant de préparer des substances pour des analyses quantitatives et qualitatives

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EP2457086A1 EP2457086A1 (fr) 2012-05-30
EP2457086B1 true EP2457086B1 (fr) 2018-02-28

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US (1) US9465017B2 (fr)
EP (1) EP2457086B1 (fr)
CH (1) CH701526B1 (fr)
DE (1) DE202010017827U1 (fr)
WO (1) WO2011010265A1 (fr)

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EP2330402B1 (fr) 2009-12-01 2017-02-15 Spark Holland B.V. Procédé et appareil pour la désorption d'un échantillon de sang d'une feuille de test médical
CH703256A1 (de) * 2010-06-04 2011-12-15 Werner Doebelin Verfahren und Vorrichtung zum automatischen und direkten analysieren von dried blood spots Proben mittels LC-MS System.
CH704174B1 (de) * 2010-11-30 2013-02-28 Camag Verfahren und Vorrichtung zur automatischen Erfassung von Substanzen für Analysen.
DE102012108158B4 (de) * 2012-09-03 2016-03-17 Johann Wolfgang Goethe-Universität Kapillarzelle, Anordnung und Verfahren zur Aufnahme, zur Positionierung und zur Untersuchung einer mikroskopischen Probe
ES2922304T3 (es) * 2012-12-20 2022-09-13 Merck Patent Gmbh Método y dispositivo para llevar a cabo cromatografía en capa fina
GB201318814D0 (en) * 2013-10-24 2013-12-11 Petroleum & Chemical Corp Microfluidic devices and arrangements for supplying such devices with reagents and biological samples
US20200341005A1 (en) 2019-04-25 2020-10-29 Euroimmun Medizinische Labordiagnostika Ag Carrier and method for detecting an analyte in dried blood spots

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Publication number Publication date
CH701526A2 (de) 2011-01-31
US9465017B2 (en) 2016-10-11
US20120125127A1 (en) 2012-05-24
WO2011010265A1 (fr) 2011-01-27
DE202010017827U1 (de) 2012-11-12
EP2457086A1 (fr) 2012-05-30
CH701526B1 (de) 2013-02-15

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